Separation device with integral guard column

• US 8,685,239 B2
• Filed: 01/11/2006
• Issued: 04/01/2014
• Est. Priority Date: 07/14/2003
• Status: Active Grant

• Current Assignee: Waters Technologies Corporation (Waters Corporation)
• Original Assignee: Waters Technologies Corporation (Waters Corporation)
• Inventors: Granger, Jennifer Harnisch, Plumb, Robert
• Primary Examiner(s): Therkorn, Ernest G
• Application Number:
  US11/329,759
• Publication Number:
  US 20060186029A1
• Time in Patent Office: 3,002 Days
• Field of Search: 210/198.2, 210/635, 210/656, 210/502.1
• US Class Current: 210/198.2
• CPC Class Codes: B01D 15/22 relating to the construction of the column
• CPC Class Codes: G01N 2030/085 using absorbing precolumn
• CPC Class Codes: G01N 30/60 Construction of the column
• CPC Class Codes: G01N 30/6039 in series
• CPC Class Codes: G01N 30/6065 with varying cross section
• CPC Class Codes: G01N 30/6069 with compartments or bed substructure

Abstract

A separation device is formed of a first tube with a cylindrical wall enclosing a chamber having a first diameter, where the device has a first end for discharging a fluid and a second end for receiving a fluid. At least two stationary phase medias are packed into the chamber with separating frits between the medias. At least one end frit element, secured to an inner surface of the first tube contains the media in its section of the chamber and allows the beds formed of the media to be formed and packed. When the separation device so constructed forms a nanocolumn with a guard bed, the guard bed may be cleaved from the separation device extending the useful life of the nanocolumn. When the separation device so constructed comprises two analytical sections, and a plurality of guard beds, complex analysis may be performed on a column having an extended useful life.

Claims

1. A separation column device comprising:

a first tube having a cylindrical wall having an inner surface defining a chamber having a first diameter, an exterior surface defining a second diameter, a first end and a second end, said first end for discharging a fluid and said second end for receiving a fluid, said chamber having a first section and a second section;

a first media contained within said first section, the first media being adapted to provide an analytical bed;

a second media contained within said second section, the second media being adapted to provide a guard bed;

a separating frit element disposed within said first tube between said first and second sections of said chamber, said separating frit element having a predesignated cleavage point at which said second section of the first tube is cleaved from the first tube after the guard bed provided by said second media has degraded from use of the separation column device, the predesignated cleavage point being located at a boundary between the separating frit element and the second section; and

an end frit element secured to said inner surface of said first tube and securing at least one of said first media in said first section and said second media in the second section in the chamber of the first tube.

2. The separation column device of claim 1 wherein said end frit element has an end aligned with one of the ends of said first tube, in order to provide minimal dead space associated with bandspreading.

3. The separation device of claim 1 wherein said first diameter is between approximately 25 μ

m and 180 μ

m.

4. The separation column device of claim 1 wherein said first tube is formed of fused silica.

5. The separation column device of claim 1 wherein said first diameter is between 70 μ

m and 110 μ

m.

6. The separating column device of claim 1 wherein said end frit element is formed as an immobilized stationary phase comprising an intimate mixture of particles comprising a stationary phase material and a polymeric network.

7. The separating column device of claim 6 wherein said polymeric network is a cross-linked poly(diorganosiloxane) and wherein said particles are suspended in said poly(diorganosiloxane).

8. The separating column device of claim 6 wherein said poly(diorganosiloxane) is polydimethelseloxane (PDMS).

9. The separating column device of claim 1 further comprising a marking on said exterior surface of said first tube indicating a location of said cleavage point of said separating frit element.

10. The separating column device of claim 1 further comprising:

an additional section in said chamber, said additional section for containing a third media; and

an additional separating frit element, said additional separating frit element disposed between said second media in said second section and said third media in said additional section.

11. The separating column device of claim 10 wherein said third media is adapted to provide a second guard bed.

12. The separating column device of claim 11 wherein one of said second media adapted to provide a guard bed and said third media adapted to provide a second guard bed is composed of a stationary phase selected from the set of ion exchange phase, reversed phase, size exclusion phase and affinity phase.

13. The separating column device of claim 1 further comprising a plurality of additional sections in the chamber separated by fit elements, each additional section being adapted to provide a guard bed, and wherein a number of additional sections adapted to provide a guard bed is between one and nine.

14. The separating column device of claim 10 wherein at least one of said first media and said third media is composed of a stationary phase selected from the set of ion exchange phase, reversed phase, size exclusion phase and affinity phase.

15. The separating column device of claim 1 wherein said separating frit element is composed of a layer of glass microspheres.

16. The separating column device of claim 15 wherein a thickness of said layer of glass microspheres is between approximately 250 and 500 μ

m.

17. The separating column device of claim 15 wherein a thickness of said layer of glass microspheres is approximately 250 μ

m.

18. The separating column device of claim 15 wherein a diameter of said glass microspheres is between approximately 3.5 and 5.0 μ

m.

19. The separating device of claim 15 wherein a diameter of said glass microspheres is approximately 5.0 μ

m.